تفاعل #10559

ord-4a6dcdf464c440f5b2372f95897642bd

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe catalyst was removed by filtration through Arbocel (trade mark) and solvent
  2. 2
    أخرىevaporated under reduced pressure
  3. 3
    أخرىThe residue was purified by column chromatography on silica gel eluting with a gradient system of dichloromethane

الإجراء التجريبي

A solution of benzyl 2-[({[2-(diisopropylamino)ethyl]amino}carbonyl)amino]ethylcarbamate (Preparation 50) (6.25 g, 14.45 mmol) in ethanol (100 ml) was hydrogenated at room temperature over palladium (II) hydroxide (250 mg) for 4 hours at 414 KPa. The catalyst was removed by filtration through Arbocel (trade mark) and solvent evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with a gradient system of dichloromethane:methanol:concentrated aqueous ammonia (90:10:1, by volume) changing to dichloromethane:methanol:concentrated aqueous ammonia (90:10:2, by volume) to afford the title compound as a yellow oil (3.6 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07094769B2uspto-grants-2006_08